#------------------------------------------------------------------------------
#$Date: 2021-03-02 10:09:29 +0200 (Tue, 02 Mar 2021) $
#$Revision: 262346 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/07/1560739.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1560739
loop_
_publ_author_name
'Gao, Wei'
'Liu, Feng'
'Zhang, Xiu-Mei'
'Liu, Jie-Ping'
'Gao, Qing-Yu'
_publ_section_title
;
 Slow relaxation and magnetic coupling of magnetization in 3D CoII2-xZnIIx
 chain-based coordination frameworks with mixed double azide-tetrazolate
 bridges
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              108
_journal_page_last               114
_journal_paper_doi               10.1016/j.jssc.2018.08.032
_journal_volume                  268
_journal_year                    2018
_chemical_formula_sum            'C10 H14 N18 O4 Zn2'
_chemical_formula_weight         581.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 116.73(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.285(14)
_cell_length_b                   10.202(8)
_cell_length_c                   13.482(11)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      3.17
_cell_volume                     2246(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0124
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17664
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.005
_diffrn_reflns_theta_max         25.005
_diffrn_reflns_theta_min         3.175
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.195
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.873
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.214
_refine_ls_extinction_coef       0.0139(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.212
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         1983
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1180P)²+25.2462P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2031
_refine_ls_wR_factor_ref         0.2076
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1836
_reflns_number_total             1983
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            JSSC-2018-268-108.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1560739
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.810
_shelx_estimated_absorpt_t_max   0.844
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 1.0000 0.30069(9) 0.7500 0.0201(4) Uani 1 2 d S T P . .
Zn2 Zn 1.0000 0.5000 1.0000 0.0153(4) Uani 1 2 d S . P . .
N1 N 0.8106(5) 0.2793(9) 0.7184(7) 0.059(2) Uani 1 1 d . . . . .
N2 N 0.8864(5) 0.3156(8) 0.7905(7) 0.056(2) Uani 1 1 d . . . . .
N3 N 0.8829(5) 0.3942(8) 0.8654(6) 0.0524(18) Uani 1 1 d . . . . .
N4 N 0.8040(4) 0.4124(8) 0.8432(6) 0.0545(19) Uani 1 1 d . . . . .
N5 N 0.5542(5) 0.2062(7) 0.5839(7) 0.0517(19) Uani 1 1 d . . . . .
N6 N 0.5405(5) 0.4200(9) 0.6440(10) 0.078(3) Uani 1 1 d . . . . .
N7 N 0.9404(5) 0.4613(9) 0.6149(7) 0.059(2) Uani 1 1 d . . . . .
N8 N 0.8996(7) 0.5430(11) 0.6316(8) 0.075(3) Uani 1 1 d . . . . .
N9 N 0.8638(11) 0.6243(16) 0.6463(13) 0.145(7) Uani 1 1 d . . . . .
O1 O 0.9394(5) 0.1341(8) 0.6282(8) 0.081(2) Uani 1 1 d . . . . .
H1B H 0.9702 0.0625 0.6514 0.122 Uiso 1 1 d R U . . .
H1C H 0.9365 0.1578 0.5623 0.122 Uiso 1 1 d R U . . .
O2 O 0.2861(13) 0.551(5) 0.5196(16) 0.48(3) Uani 1 1 d D . . . .
H2A H 0.237(9) 0.54(5) 0.51(3) 0.724 Uiso 1 1 d D U . . .
H2B H 0.295(16) 0.51(4) 0.47(2) 0.724 Uiso 1 1 d D U . . .
C1 C 0.7617(5) 0.3418(9) 0.7520(8) 0.049(2) Uani 1 1 d . . . . .
C4 C 0.5090(6) 0.3088(10) 0.5895(10) 0.066(3) Uani 1 1 d . . . . .
H4 H 0.4522 0.3011 0.5529 0.079 Uiso 1 1 calc R U . . .
C3 C 0.6218(6) 0.4311(11) 0.6953(10) 0.067(3) Uani 1 1 d . . . . .
H3 H 0.6448 0.5086 0.7328 0.080 Uiso 1 1 calc R U . . .
C2 C 0.6731(6) 0.3328(9) 0.6952(8) 0.052(2) Uani 1 1 d . . . . .
C5 C 0.6344(5) 0.2204(9) 0.6332(8) 0.051(2) Uani 1 1 d . . . . .
H5 H 0.6667 0.1536 0.6269 0.061 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Zn1 O1 83.3(5) . 2_756
O1 Zn1 N7 175.2(3) . 2_756
O1 Zn1 N7 93.3(3) 2_756 2_756
O1 Zn1 N7 93.3(3) . .
O1 Zn1 N7 175.2(3) 2_756 .
N7 Zn1 N7 90.4(5) 2_756 .
O1 Zn1 N2 94.3(3) . 2_756
O1 Zn1 N2 91.2(3) 2_756 2_756
N7 Zn1 N2 89.1(3) 2_756 2_756
N7 Zn1 N2 85.7(3) . 2_756
O1 Zn1 N2 91.2(3) . .
O1 Zn1 N2 94.3(3) 2_756 .
N7 Zn1 N2 85.7(3) 2_756 .
N7 Zn1 N2 89.1(3) . .
N2 Zn1 N2 172.7(4) 2_756 .
N7 Zn2 N7 180.0 6_566 2_756
N7 Zn2 N3 86.8(3) 6_566 5_767
N7 Zn2 N3 93.2(3) 2_756 5_767
N7 Zn2 N3 93.2(3) 6_566 .
N7 Zn2 N3 86.8(3) 2_756 .
N3 Zn2 N3 180.0 5_767 .
N7 Zn2 N5 93.1(3) 6_566 8_556
N7 Zn2 N5 86.9(3) 2_756 8_556
N3 Zn2 N5 89.9(3) 5_767 8_556
N3 Zn2 N5 90.1(3) . 8_556
N7 Zn2 N5 86.9(3) 6_566 4_656
N7 Zn2 N5 93.1(3) 2_756 4_656
N3 Zn2 N5 90.1(3) 5_767 4_656
N3 Zn2 N5 89.9(3) . 4_656
N5 Zn2 N5 180.0 8_556 4_656
C1 N1 N2 104.8(7) . .
N3 N2 N1 109.6(7) . .
N3 N2 Zn1 124.4(6) . .
N1 N2 Zn1 122.8(6) . .
N2 N3 N4 109.3(7) . .
N2 N3 Zn2 122.0(6) . .
N4 N3 Zn2 128.3(6) . .
C1 N4 N3 104.5(7) . .
C5 N5 C4 117.1(8) . .
C5 N5 Zn2 117.8(6) . 4_646
C4 N5 Zn2 125.0(6) . 4_646
C3 N6 C4 117.6(9) . .
N8 N7 Zn2 121.9(8) . 2_756
N8 N7 Zn1 116.9(7) . .
Zn2 N7 Zn1 116.9(3) 2_756 .
N9 N8 N7 176.4(17) . .
Zn1 O1 H1B 109.6 . .
Zn1 O1 H1C 107.8 . .
H1B O1 H1C 108.4 . .
H2A O2 H2B 112.00 . .
N4 C1 N1 111.9(8) . .
N4 C1 C2 124.7(8) . .
N1 C1 C2 123.4(8) . .
N6 C4 N5 124.3(9) . .
N6 C4 H4 117.9 . .
N5 C4 H4 117.9 . .
N6 C3 C2 122.7(9) . .
N6 C3 H3 118.7 . .
C2 C3 H3 118.7 . .
C3 C2 C5 115.7(9) . .
C3 C2 C1 123.7(9) . .
C5 C2 C1 120.6(8) . .
N5 C5 C2 122.5(9) . .
N5 C5 H5 118.8 . .
C2 C5 H5 118.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 2.275(8) .
Zn1 O1 2.275(8) 2_756
Zn1 N7 2.325(9) 2_756
Zn1 N7 2.325(9) .
Zn1 N2 2.378(8) 2_756
Zn1 N2 2.379(8) .
Zn2 N7 2.294(8) 6_566
Zn2 N7 2.294(8) 2_756
Zn2 N3 2.355(8) 5_767
Zn2 N3 2.355(8) .
Zn2 N5 2.383(7) 8_556
Zn2 N5 2.383(7) 4_656
N1 C1 1.333(12) .
N1 N2 1.338(11) .
N2 N3 1.314(11) .
N3 N4 1.348(10) .
N4 C1 1.332(12) .
N5 C5 1.318(12) .
N5 C4 1.357(12) .
N5 Zn2 2.383(7) 4_646
N6 C3 1.333(13) .
N6 C4 1.333(13) .
N7 N8 1.205(12) .
N7 Zn2 2.294(8) 2_756
N8 N9 1.128(14) .
O1 H1B 0.8885 .
O1 H1C 0.8988 .
O2 H2A 0.850(11) .
O2 H2B 0.850(10) .
C1 C2 1.449(12) .
C4 H4 0.9300 .
C3 C2 1.374(14) .
C3 H3 0.9300 .
C2 C5 1.408(13) .
C5 H5 0.9300 .
